GB/T 37505-2019 PDF English
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Surface active agents - Determination of quinoline content in dispersing agents
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GB/T 37505-2019: PDF in English (GBT 37505-2019) GB/T 37505-2019
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
G 72
Surface active agents - Determination of quinoline
content in dispersing agents
ISSUED ON: JUNE 04, 2019
IMPLEMENTED ON: MAY 01, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle ... 4
4 Reagents ... 4
5 Instruments and devices ... 5
6 Determination methods ... 6
7 Detection limit, recovery rate and precision ... 10
8 Test report ... 11
Annex A (informative) GC-FID chromatogram of quinoline standard product 12
Annex B (informative) GC-MS total ion chromatogram and mass spectrum of
quinoline standard product ... 13
Surface active agents - Determination of quinoline
content in dispersing agents
1 Scope
This Standard specifies the determination method for quinoline content in
surface active dispersing agents.
This Standard is applicable to various surface-active dispersing agents that are
produced from coal chemical raw materials.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
GB/T 8170, Rules of rounding off for numerical values & expression and
judgement of limiting values
GB/T 9722-2006, Chemical reagent - General rules for the gas
chromatography
3 Principle
Disperse and dissolve the sample in water. Use ethyl acetate to extract the
quinoline in it. Use gas chromatography or gas chromatography-mass
spectrometry to detect. Use peak area external standard method to quantify.
4 Reagents
4.1 General provisions
Unless otherwise stated, use analytical reagents that meet national standards.
The test water shall meet the specifications for grade three water in GB/T 6682.
5.7 Organic phase needle filter
The specification is 13mm × 0.45μm.
5.8 Pipette
The capacity is 20mL.
6 Determination methods
6.1 Sample pre-treatment
Weigh 0.5g of sample (to the nearest of 0.0001g). Place in the extractor (see
5.6). Add 20mLof water. Shake vigorously till dissolved or fully wetted and
dispersed. Use the pipette (see 5.8) to accurately add 20mL of ethyl acetate
(see 4.2). Shake the extractor for 0.5min to make the aqueous phase and the
organic phase fully contact. It may also use ultrasonic-assisted extraction.
Conduct static layering (if the emulsification is serious and the layering is slower,
it can be centrifuged at 3000r/min for 10min). Take the supernatant. For the
sample solution that is filtered through the organic phase needle filter (see 5.7),
use gas chromatograph or GC/MS to analyze. If the sample concentration
exceeds the linear range of the instrument, it needs to dilute the sample to the
linear range.
6.2 Gas chromatography
6.2.1 Gas chromatography analysis conditions
Since the test results depend on the instrument used, it is not possible to give
general parameters for chromatographic analysis. It may choose the best
analysis conditions according to different equipment. Use the following
parameters that have been proved suitable for the test. The parameters are as
follows:
- Chromatographic column: HP-5, 30m × 0.32mm × 0.25μm, or equivalent;
- Carrier gas: nitrogen, constant flow, flow rate of 1mL/min;
- Inlet temperature: 270°C;
- Detector (FID) temperature: 300°C;
- Hydrogen flow: 40mL/min;
- Air flow: 400mL/min;
- Compensation gas: nitrogen, 30mL/min;
milligrams per kilogram (mg/kg):
Where,
A - Peak area of quinoline in sample solution;
V - Volume of sample solution, in milliliters (mL);
a, b - Standard curve constants;
m - Sample mass, in grams (g);
F - Dilution factor.
The calculation result is rounded off to the integer according to GB/T 8170.
6.3 Gas chromatography-mass spectrometry (arbitration method)
6.3.1 GC-MS analysis conditions
Since the test results depend on the instrument used, it is not possible to give
general parameters for chromatographic analysis. It may choose the best
analysis conditions according to different equipment. Use the following
parameters that have been proved suitable for the test. The parameters are as
follows:
- Chromatographic column: HP-5MS, 30m × 0.25mm × 0.25μm, or
equivalent;
- Carrier gas: nitrogen, constant flow, flow rate of 1mL/min;
- Inlet temperature: 260°C;
- Auxiliary interface temperature: 280°C;
- Injection volume: 1μL;
- Injection method: injection without flow division;
- Heating program: maintain at 80°C for 2min, rise at 10°C/min to 180°C for
2min;
- Solvent delay: 4min;
- Ion source temperature: 230°C;
Where,
A - Quinoline quantitative ion peak area;
c - Quinoline concentration, in milligrams per liter (mg/L);
a, b - Standard curve constants.
After each instrument maintenance or replacement of parts, it shall redraw the
standard curve. It is recommended that before each test of sample solution, use
the quinoline standard solution with a known concentration to verify the curve.
When the error exceeds 5%, it shall redraw the standard curve.
6.3.4 Sample determination steps
Analyze the sample solution that has been well processed according to the
chromatographic conditions (see 6.3.1). Record the quinoline quantitative ion
peak area A in the sample solution.
6.3.5 Result calculation
The quinoline content in surface active agent is calculated according to formula
(4).
The quinoline content X in surface active agent is calculated according to
formula (4), in milligrams per kilogram (mg/kg):
A - Peak area of quinoline quantifier ion in sample solution;
V - Volume of extract liquid, in milliliters (mL);
a, b - Standard curve constants;
m - Sample mass, in grams (g);
F - Dilution factor.
The calculation result is rounded off to the integer according to GB/T 8170.
7 Detection limit, recovery rate and precision
7.1 Detection limit
GC-FID detection limit is 20mg/kg. GC-MS detection limit is 5mg/kg.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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